CN102220686B - Method for improving degradation property of silk threads, and modified degummed silk threads - Google Patents
Method for improving degradation property of silk threads, and modified degummed silk threads Download PDFInfo
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- CN102220686B CN102220686B CN201110115064.2A CN201110115064A CN102220686B CN 102220686 B CN102220686 B CN 102220686B CN 201110115064 A CN201110115064 A CN 201110115064A CN 102220686 B CN102220686 B CN 102220686B
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Abstract
The invention provides a processing method of degummed silk threads. The processing method comprises that degummed silk threads are radiated by gamma rays in the absence of oxygen, wherein an irradiation dose is in a range of 50 to 1000 kGy. The invention also provides modified degummed silk threads obtained by the above processing method. The modified degummed silk threads have a good mechanical property and a good degradation property, and are suitable as sutures, nerve conduits, artificial blood vessels or artificial bones.
Description
Technical field
The present invention relates to technical field of biological material, particularly a kind of method and modified silk boiled-off silk line that improves silk line degradation property.
Background technology
Bombyx mori silk fibroin fiber, claims again silk fiber, is a kind of natural polymer, and it is by the synthetic natural animal albumen with excellent mechanical performances with secreting of silk glands of silkworm, conventionally by silk, through degumming process, is obtained.The protein that fibroin fiber is comprised of 20 seed amino acids that can be absorbed by organism, fibroin fiber itself should have biocompatibility in theory, and catabolite is nontoxic, has no side effect, and can be absorbed by human body, and have excellent mechanical property.Therefore, fibroin fiber is more and more subject to the extensive concern of medical domain and Material Field, is expected to as embedded materials such as regeneration support or fillers.
As medical material, embedded material especially, the degradation rate that should there is degradability and match with organization healing speed after material implants.And fibroin fiber belongs to crystallization high polymer, its crystal region content is about 45%～55%, crystal region and noncrystalline domain alternative arrangement, hard degradation.According to American Pharmacopeia (USP), define, degradation material refers to implant and within 60 days, loses the material of nearly all TENSILE STRENGTH, and generally in fibroin fiber implantable bioartificial body, within approximately 1 year, just can lose most of TENSILE STRENGTH, implant and in transplanting place, be beyond recognition (Somerville after 2 years, NJ:Ethicon, Inc. (copyright 2000, and Chapter 2)).There is many documents confirm the to know clearly weak degradation capability of silk fiber both at home and abroad.For example Greenwald D et al. has reported that fibroin fiber implantation mouse skin histology is after 6 weeks, and TENSILE STRENGTH still keeps 45%, and elastic modelling quantity decline 16% (JSurg Res, 1994,56:372).Lam KH et al. reported fibroin suture implanted to mouse after 6 weeks, and fibrous fracture can not be taken out from implant site, after 24 weeks, can't detect fibroin fiber (JAppl Biomater, 1995,6:191).The nerve-grafting material that and for example Yang YM et al. is prepared do filling with fibroin fiber has good mechanical property and biocompatibility, by proteasome degradation, test, within 24 weeks, degraded 79% (Polymer Degradation and Stability, 2009,94:2213).Hence one can see that, fibroin fiber belong to difficult degradation material (Biomaterials, 2003,24:401).If material is implanted, material can not, by the human body absorption of effectively degrading, easily cause organism rejection, and then bring out infection, even threat to life.Therefore, the low degradability of fibroin fiber has a strong impact on it as the application of embedded material.
In order to improve the degradation property of silk fibroin material, prior art is normally dissolved silk fiber, prepares regenerated silk fibroin material as film, porous support, regulates the degradation property of silk fibroin material, as.For example, Wang Y Z et al. has reported by changing concentration, the solvent of silk fibroin protein solution, regulates the aperture of material, can obtain the silk fibroin porous material (Biomaterials of different degradation capabilities (degradation speed), 2008,29:3415).But the mechanical property of materials that said method is made is not ideal enough, has much room for improvement, also limited thus the range of application of silk fibroin material.
Silk boiled-off silk line consists of fibroin fiber, has good mechanical property, and the inventor considers silk boiled-off silk line to process to improve its degradation capability thus, to obtain the silk thread with excellent mechanical property and degradation property.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of processing method of silk boiled-off silk line, processes the modified silk boiled-off silk line obtaining have good degradation capability by the method, also keeps good mechanical property simultaneously.
In view of this, the invention provides a kind of processing method of silk boiled-off silk line, comprising:
Under oxygen free condition, silk boiled-off silk line is carried out to gamma-radiation irradiation, the dosage of described irradiation is 50kGy～1000kGy.
Preferably, the preparation method of described silk boiled-off silk line is:
Silk line is carried out to degumming process, obtain silk boiled-off silk line.
Preferably, the preparation method of described silk line is:
By some silkworm raw silk twisting, obtain silk line.
Preferably, described degumming process is specially:
A), use sodium carbonate liquor to process silk line 1～3 time, treatment temperature is 95 ℃～100 ℃;
B), silk line that step a is obtained washes successively, draws pine, dry.
Preferably, described oxygen free condition is vacuum.
Preferably, also comprise:
Modified silk boiled-off silk line after irradiation is placed in to ventilation 12h～36h.
The present invention also provides a kind of and obtains modified silk boiled-off silk line according to above-mentioned processing method.
The processing method that the invention provides a kind of silk boiled-off silk line, is specially: under oxygen free condition, silk boiled-off silk line is carried out to gamma-radiation irradiation, the dosage of irradiation is 50kGy～1000kGy.The present invention is that to take silk boiled-off silk line be raw material, silk boiled-off silk line has higher fracture strength and elongation at break, it is carried out under oxygen free condition to gamma-radiation irradiation, by controlling, when suitable irradiation dose makes silk boiled-off silk line improve degradation property, keep good mechanical property.The modified silk boiled-off silk line that the present invention obtains after processing has good degradation property and keeps good mechanical property, is suitable as operation suture thread, nerve trachea, artificial blood vessel or artificial bone etc.
The specific embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The processing method that the embodiment of the invention discloses a kind of silk boiled-off silk line, comprising: under oxygen free condition, silk boiled-off silk line is carried out to gamma-radiation irradiation, the dosage of described irradiation is 50kGy～1000kGy.
Said method is that to take silk boiled-off silk line be raw material, and silk boiled-off silk line is the silk threads that form after some rhizoid cellulose fibers twisting.Fibroin fiber is added to the silk boiled-off silk line mechanical property being twisted into excellent, there is higher fracture strength and elongation at break.
Consider to be difficult to add after single silk fiber degumming process to be twisted into silk thread, so the silk boiled-off silk line that the present invention uses preferably undertakies obtaining after degumming process by silk line, after silk line degumming process, still can keep yarn shape.Silk line can be prepared as follows: by some raw silk twisting, obtain silk yarn.Radical those skilled in the art for raw silk in silk line can select according to the mechanical property of expected product, and the silk thread intensity that silk radical more obtains after multiprocessing is better.
A), silk line preferably carries out degumming process in the following manner:
Use sodium carbonate liquor to process silk line 1～3 time, treatment temperature is 95 ℃～100 ℃;
B), silk line that step a is obtained washes successively, draws pine, dry.
In above-mentioned degumming process, the concentration of the sodium carbonate liquor using is preferably 0.2g/L～0.3g/L, 0.25g/L more preferably; bath raio is preferably: 0.15kg silk line/10L solution; treatment temperature is preferably 98 ℃～100 ℃; number of processes is preferably 3 times, each processing time is preferably 30 minutes～and 45 minutes.After processing, wash again successively, La Song and dry, baking temperature is preferably 50 ℃～65 ℃, just completes Degumming Procedures after dry, makes silk boiled-off silk line.
The object that the present invention carries out gamma-radiation irradiation by silk boiled-off silk line is to improve the degradation property of silk boiled-off silk line.Irradiation need to carry out under oxygen free condition, this be because: oxygen can be oxidized fibroin fiber, and under the condition of equal irradiation dose, aerobic state can make the easier yellowing of fibroin fiber, and the mechanical property range of decrease is obvious.The present invention preferably carries out gamma-radiation irradiation by silk boiled-off silk line under vacuum condition.
The irradiation dose of gamma-radiation irradiation has material impact to mechanical property and the degradation property of the modified silk boiled-off silk line after processing.The degradation property of fibroin fiber promotes along with the increase of irradiation dose, and its mechanical property reduces along with the increase of irradiation dose.Irradiation dose is too low, and fibroin fiber degradation property promotes not obvious, still cannot be applied to embedded material; Irradiation dose is too high, and mechanical property that can heavy damage fiber, cannot apply it.Therefore to control irradiation dose be 50kGy～1000kGy in the present invention, and the modified silk boiled-off silk line obtaining after the irradiation dose of this scope is processed has the improvement of the different gradients of degradation property, has again and be applicable to the mechanical property used.After irradiation, also preferably modified silk boiled-off silk line is placed in to ventilation 12h～36h.
From said method, the present invention is that to take silk boiled-off silk line be raw material, it is carried out under oxygen free condition to gamma-radiation irradiation, keeps good mechanical property by controlling when suitable irradiation dose makes silk boiled-off silk line improve degradation property simultaneously.
The present invention also provides a kind of modified silk boiled-off silk line obtaining of processing according to the method described above, and this modified silk boiled-off silk line has good degradation property and mechanical property.
In order further to understand the present invention, below in conjunction with embodiment, processing method provided by the invention is described, protection scope of the present invention is not limited by the following examples.
Embodiment 1
1, will after 8～10 20/22 silkworm raw silk twisting, obtain silk line, take 0.15kg silk line and put into the aqueous sodium carbonate that 10L concentration is 0.25g/L, at 98 ℃～100 ℃, process three times, water in the aqueous sodium carbonate of front twice use is running water, each processing 30 minutes, water in the aqueous sodium carbonate using is for the third time deionized water, and the processing time is 45 minutes.Then with deionized water, silk line is fully rinsed well, drawn pine, be placed in 60 ℃ of baking oven inner dryings, complete Degumming Procedures, obtain silk boiled-off silk line.
2, silk boiled-off silk line step 1 being made is placed in radiotolerant metallic aluminium pool, vacuumize processing, discharge the air in metallic aluminium pool, sealing metal aluminium pool is communicated with to inner silk boiled-off silk line and carries out gamma-radiation radiation treatment, irradiation dose is 50kGy, after irradiation, modified silk boiled-off silk line is taken out, under ventilation state, place 24 hours.
Adopt the silk boiled-off silk line mechanical property after Instrong3365 universal material experimental machine test predose, the fracture strength and the elongation at break that record the modified silk boiled-off silk line after irradiation are respectively 95% and 98% of predose.
Get the modified silk boiled-off silk line through radiation treatment of identical weight and without the silk boiled-off silk line of irradiation, all with the bath raio of 1: 100, put into 0.5mg/ml Collagenase IA solution, be placed in 37 ℃ of water-baths vibration 36 days, during within every three days, change the once Collagenase IA solution of new configuration.After 36 days, elimination Collagenase IA solution, deionized water washing 3 times for catabolite, remove residual Collagenase, oven dry is weighed, calculate: the modified silk boiled-off silk line enzyme degraded dissolve-loss ratio after irradiation is 13.70%, and the silk boiled-off silk line enzyme of irradiation degraded dissolve-loss ratio is not 12.46%, and the degradation capability of irradiation post-modification silk boiled-off silk line improves approximately 10%.
Embodiment 2
1, will after 8～10 20/22 silkworm raw silk twisting, obtain silk line, take 0.15kg silk line and put into the aqueous sodium carbonate that 10L concentration is 0.25g/L, at 98 ℃～100 ℃, process three times, water in the aqueous sodium carbonate of front twice use is running water, each processing 30 minutes, water in the aqueous sodium carbonate using is for the third time deionized water, and the processing time is 45 minutes.Then with deionized water, silk line is fully rinsed well, drawn pine, be placed in 60 ℃ of baking oven inner dryings, complete Degumming Procedures, obtain silk boiled-off silk line.
2, silk boiled-off silk line step 1 being made is placed in radiotolerant metallic aluminium pool, vacuumize processing, discharge the air in metallic aluminium pool, sealing metal aluminium pool is communicated with to inner silk boiled-off silk line and carries out gamma-radiation radiation treatment, irradiation dose is 100kGy, after irradiation, modified silk boiled-off silk line is taken out, under ventilation state, place 24 hours.
Adopt the silk boiled-off silk line mechanical property after Instrong3365 universal material experimental machine test predose, the fracture strength and the elongation at break that record the modified silk boiled-off silk line after irradiation are respectively 90% and 85% of predose.
Get the modified silk boiled-off silk line through radiation treatment of identical weight and without the silk boiled-off silk line of irradiation, all with the bath raio of 1: 100, put into 0.5mg/ml Collagenase IA solution, be placed in 37 ℃ of water-baths vibration 36 days, during within every three days, change the once Collagenase IA solution of new configuration.After 36 days, elimination Collagenase IA solution, deionized water washing 3 times for catabolite, remove residual Collagenase, oven dry is weighed, calculate: the modified silk boiled-off silk line enzyme degraded dissolve-loss ratio after irradiation is 15.59%, and the silk boiled-off silk line enzyme of irradiation degraded dissolve-loss ratio is not 12.46%, and the degradation capability of irradiation post-modification silk boiled-off silk line improves approximately 25%.
Embodiment 3
1, will after 8～10 20/22 silkworm raw silk twisting, obtain silk line, take 0.15kg silk line and put into the aqueous sodium carbonate that 10L concentration is 0.25g/L, at 98 ℃～100 ℃, process three times, water in the aqueous sodium carbonate of front twice use is running water, each processing 30 minutes, water in the aqueous sodium carbonate using is for the third time deionized water, and the processing time is 45 minutes.Then with deionized water, silk line is fully rinsed well, drawn pine, be placed in 60 ℃ of baking oven inner dryings, complete Degumming Procedures, obtain silk boiled-off silk line.
2, silk boiled-off silk line step 1 being made is placed in radiotolerant metallic aluminium pool, vacuumize processing, discharge the air in metallic aluminium pool, sealing metal aluminium pool is communicated with to inner silk boiled-off silk line and carries out gamma-radiation radiation treatment, irradiation dose is 200kGy, after irradiation, modified silk boiled-off silk line is taken out, under ventilation state, place 24 hours.
Adopt the silk boiled-off silk line mechanical property after Instrong3365 universal material experimental machine test predose, the fracture strength and the elongation at break that record the modified silk boiled-off silk line after irradiation are respectively 80% and 70% of predose.
Get the modified silk boiled-off silk line through radiation treatment of identical weight and without the silk boiled-off silk line of irradiation, all with the bath raio of 1: 100, put into 0.5mg/ml Collagenase IA solution, be placed in 37 ℃ of water-baths vibration 36 days, during within every three days, change the once Collagenase IA solution of new configuration.After 36 days, elimination Collagenase IA solution, deionized water washing 3 times for catabolite, remove residual Collagenase, oven dry is weighed, calculate: the modified silk boiled-off silk line enzyme degraded dissolve-loss ratio after irradiation is 16.85%, and the silk boiled-off silk line enzyme of irradiation degraded dissolve-loss ratio is not 12.46%, and the degradation capability of irradiation post-modification silk boiled-off silk line improves approximately 35%.
Embodiment 4
1, will after 8～10 20/22 silkworm raw silk twisting, obtain silk line, take 0.15kg silk line and put into the aqueous sodium carbonate that 10L concentration is 0.25g/L, at 98 ℃～100 ℃, process three times, water in the aqueous sodium carbonate of front twice use is running water, each processing 30 minutes, water in the aqueous sodium carbonate using is for the third time deionized water, and the processing time is 45 minutes.Then with deionized water, silk line is fully rinsed well, drawn pine, be placed in 60 ℃ of baking oven inner dryings, complete Degumming Procedures, obtain silk boiled-off silk line.
2, silk boiled-off silk line step 1 being made is placed in radiotolerant metallic aluminium pool, vacuumize processing, discharge the air in metallic aluminium pool, sealing metal aluminium pool is communicated with to inner silk boiled-off silk line and carries out gamma-radiation radiation treatment, irradiation dose is 500kGy, after irradiation, modified silk boiled-off silk line is taken out, under ventilation state, place 24 hours.
Adopt the silk boiled-off silk line mechanical property after Instrong3365 universal material experimental machine test predose, the fracture strength and the elongation at break that record the modified silk boiled-off silk line after irradiation are respectively 65% and 50% of predose.
Get the modified silk boiled-off silk line through radiation treatment of identical weight and without the silk boiled-off silk line of irradiation, all with the bath raio of 1: 100, put into 0.5mg/ml Collagenase IA solution, be placed in 37 ℃ of water-baths vibration 36 days, during within every three days, change the once Collagenase IA solution of new configuration.After 36 days, elimination Collagenase IA solution, deionized water washing 3 times for catabolite, remove residual Collagenase, oven dry is weighed, calculate: the modified silk boiled-off silk line enzyme degraded dissolve-loss ratio after irradiation is 19.29%, and the silk boiled-off silk line enzyme of irradiation degraded dissolve-loss ratio is not 12.46%, and the degradation capability of irradiation post-modification silk boiled-off silk line improves approximately 55%.
Embodiment 5
1, will after 8～10 20/22 silkworm raw silk twisting, obtain silk line, take 0.15kg silk line and put into the aqueous sodium carbonate that 10L concentration is 0.25g/L, at 98 ℃～100 ℃, process three times, water in the aqueous sodium carbonate of front twice use is running water, each processing 30 minutes, water in the aqueous sodium carbonate using is for the third time deionized water, and the processing time is 45 minutes.Then with deionized water, silk line is fully rinsed well, drawn pine, be placed in 60 ℃ of baking oven inner dryings, complete Degumming Procedures, obtain silk boiled-off silk line.
2, silk boiled-off silk line step 1 being made is placed in radiotolerant metallic aluminium pool, vacuumize processing, discharge the air in metallic aluminium pool, sealing metal aluminium pool is communicated with to inner silk boiled-off silk line and carries out gamma-radiation radiation treatment, irradiation dose is 1000kGy, after irradiation, modified silk boiled-off silk line is taken out, under ventilation state, place 24 hours.
Adopt the silk boiled-off silk line mechanical property after Instrong3365 universal material experimental machine test predose, the fracture strength and the elongation at break that record the modified silk boiled-off silk line after irradiation are respectively 40% and 25% of predose.
Get the modified silk boiled-off silk line through radiation treatment of identical weight and without the silk boiled-off silk line of irradiation, all with the bath raio of 1: 100, put into 0.5mg/ml Collagenase IA solution, be placed in 37 ℃ of water-baths vibration 36 days, during within every three days, change the once Collagenase IA solution of new configuration.After 36 days, elimination Collagenase IA solution, deionized water washing 3 times for catabolite, remove residual Collagenase, oven dry is weighed, calculate: the modified silk boiled-off silk line enzyme degraded dissolve-loss ratio after irradiation is 24.93%, and the silk boiled-off silk line enzyme of irradiation degraded dissolve-loss ratio is not 12.46%, and the degradation capability of irradiation post-modification silk boiled-off silk line improves approximately 100%.
Comparative example 1
1, will after 8～10 20/22 silkworm raw silk twisting, obtain silk line, take 0.15kg silk line and put into the aqueous sodium carbonate that 10L concentration is 0.25g/L, at 98 ℃～100 ℃, process three times, water in the aqueous sodium carbonate of front twice use is running water, each processing 30 minutes, water in the aqueous sodium carbonate using is for the third time deionized water, and the processing time is 45 minutes.Then with deionized water, silk line is fully rinsed well, drawn pine, be placed in 60 ℃ of baking oven inner dryings, complete Degumming Procedures, obtain silk boiled-off silk line.
2, silk boiled-off silk line step 1 being made is placed in radiotolerant metallic aluminium pool, vacuumize processing, discharge the air in metallic aluminium pool, sealing metal aluminium pool is communicated with to inner silk boiled-off silk line and carries out gamma-radiation radiation treatment, irradiation dose is 2000kGy, after irradiation, modified silk boiled-off silk line is taken out, under ventilation state, place 24 hours.
Adopt the silk boiled-off silk line mechanical property after Instrong3365 universal material experimental machine test predose, the fracture strength and the elongation at break that record the modified silk boiled-off silk line after irradiation are respectively 6% and 20% of predose, and mechanical property is poor, is difficult to application.
Comparative example 2
1, will after 8～10 20/22 silkworm raw silk twisting, obtain silk line, take 0.15kg silk line and put into the aqueous sodium carbonate that 10L concentration is 0.25g/L, at 98 ℃～100 ℃, process three times, water in the aqueous sodium carbonate of front twice use is running water, each processing 30 minutes, water in the aqueous sodium carbonate using is for the third time deionized water, and the processing time is 45 minutes.Then with deionized water, silk line is fully rinsed well, drawn pine, be placed in 60 ℃ of baking oven inner dryings, complete Degumming Procedures, obtain silk boiled-off silk line.
2, silk boiled-off silk line step 1 being made is placed in radiotolerant metallic aluminium pool, vacuumize processing, discharge the air in metallic aluminium pool, sealing metal aluminium pool is communicated with to inner silk boiled-off silk line and carries out gamma-radiation radiation treatment, irradiation dose is 3000kGy, after irradiation, modified silk boiled-off silk line is taken out, under ventilation state, place 24 hours.
Adopt the silk boiled-off silk line mechanical property after Instrong3365 universal material experimental machine test predose, the fracture strength and the elongation at break that record the modified silk boiled-off silk line after irradiation are 0, as silk thread, there is no actual application value.
From the above results, the degradation property of silk boiled-off silk line improves along with the increase of irradiation dose, mechanical property reduces along with the increase of irradiation dose, irradiation dose is that the modified silk boiled-off silk line after 50～1000 processing just has good degradation property, when irradiation dose surpasses 1000, modified silk boiled-off silk line mechanical property after processing is poor, and using value is low.The modified silk boiled-off silk line that the present invention obtains after processing has good mechanics and degradation property, is suitable as operation suture thread, nerve trachea, artificial blood vessel or artificial bone etc.
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Above-mentioned explanation to the disclosed embodiments, makes professional and technical personnel in the field can realize or use the present invention.To the multiple modification of these embodiment, will be apparent for those skilled in the art, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (2)
1. a processing method for silk boiled-off silk line, is characterized in that, comprising:
Under oxygen free condition, silk boiled-off silk line is carried out to gamma-radiation irradiation, the dosage of described irradiation is 50kGy～1000kGy;
Modified silk boiled-off silk line after irradiation is placed in to ventilation 12h～36h;
Wherein, described oxygen free condition is vacuum;
The preparation method of described silk boiled-off silk line is:
By some silkworm raw silk twisting, obtain silk line;
Silk line is carried out to degumming process: use sodium carbonate liquor to process silk line 1～3 time, treatment temperature is 95 ℃～100 ℃, then the silk line obtaining is washed successively, draws pine, dry, obtains silk boiled-off silk line.
2. according to processing method claimed in claim 1, obtain modified silk boiled-off silk line.
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| KR101570717B1 (en) * | 2014-08-04 | 2015-11-24 | 대한민국 | Dental Membrain using Cocoon and Method for manufacturing thereof |
| CN104592659A (en) * | 2015-01-31 | 2015-05-06 | 安徽弘毅电缆集团有限公司 | Cold-resistant modified composite cable sheathing material |
| CN104592658A (en) * | 2015-01-31 | 2015-05-06 | 安徽弘毅电缆集团有限公司 | Cold-resistant cable sheathing material |
| CN110042654B (en) * | 2019-05-22 | 2022-02-11 | 广西柳城县鹏翔茧丝绸有限责任公司 | High-light-resistance silk fabric and preparation method thereof |
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